WO2016176922A1 - Batterie secondaire au lithium-iode à système de solution électrolytique organique et son procédé de fabrication - Google Patents

Batterie secondaire au lithium-iode à système de solution électrolytique organique et son procédé de fabrication Download PDF

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WO2016176922A1
WO2016176922A1 PCT/CN2015/086440 CN2015086440W WO2016176922A1 WO 2016176922 A1 WO2016176922 A1 WO 2016176922A1 CN 2015086440 W CN2015086440 W CN 2015086440W WO 2016176922 A1 WO2016176922 A1 WO 2016176922A1
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iodine
lithium
secondary battery
organic electrolyte
electrolyte system
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PCT/CN2015/086440
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English (en)
Chinese (zh)
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陈军
赵庆
卢艳莹
陶占良
朱智强
胡宇翔
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南开大学
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to an organic electrolyte system lithium iodine secondary battery and a preparation method thereof, in particular to an organic electrolyte system lithium iodine secondary battery using iodine element/carbon composite material as a positive electrode and a preparation method thereof.
  • Lithium-iodine solid-state electrolyte primary batteries have been used in cardiac pacemaker power supplies since 1972 due to their high energy density, high reliability, and low self-discharge (JRMoser, US Patent, 3, 660, 163).
  • JRMoser US Patent, 3, 660, 163
  • this type of battery has a large internal resistance during discharge, and the rate performance is greatly limited.
  • the capacity will still decay with the cycle.
  • the specific discharge capacity was attenuated from -400 mAh/g to less than 250 mAh/g.
  • the iodine dissolved in the electrolyte will flow to the negative electrode side and directly react with lithium, resulting in a strong self-discharge phenomenon.
  • the specific discharge capacity was reduced from ⁇ 250 mAh/g to ⁇ 200 mAh/g.
  • Their positive electrode material is a synthetic method using conventional heat treatment.
  • the iodine element and the carbon material are simultaneously added to the inner tank of the polytetrafluoroethylene, and after sealing, the mixture is heated to 200 ° C so that the iodine element becomes iodine vapor and penetrates into the carbon material.
  • iodine vapor is attached to the inner wall of the inner liner and the surface of the carbon material, causing loss of raw materials, and the iodine attached to the surface of the carbon material needs to be removed through a washing process, and the preparation process is complicated, and the load is difficult to control.
  • the object of the present invention is to provide an organic electrolyte system lithium iodine secondary battery and a preparation method thereof, which can overcome the problems of serious self-discharge in the lithium ion iodine secondary battery of the current organic electrolyte system and complicated preparation of the positive electrode material.
  • the lithium-iodine secondary battery of the organic electrolyte system of the invention has long cycle life, high rate performance, low self-discharge effect and strong practicability
  • the method has the advantages of low preparation cost, simple process, good electrochemical performance, safety and pollution-free, and has wide application prospects.
  • the organic electrolyte system provided by the present invention comprises a positive electrode, a negative electrode, a separator, and an organic electrolyte containing an additive.
  • the positive electrode material comprises an iodine elemental/carbon composite active material, wherein the iodine content is 10% to 80% (mass fraction).
  • the preparation method of the iodine element/carbon composite material adopts a dissolution-adsorption method, and the steps include:
  • the carbon material is one or two of porous carbon materials having high specific surface area, high porosity and high electrical conductivity, such as activated carbon cloth, activated carbon, CMK-3, porous conductive carbon black, ordered mesoporous carbon, and the like. Mixture of any of the above ratios.
  • the mass ratio of the iodine element to the carbon material is 1:9-8:2.
  • the negative electrode is a metallic lithium or a lithium-containing alloy.
  • the separator is a three-layer composite film composed of polyethylene, polypropylene, and polyethylene in sequence, a Celgard series film (Celgard 2340) or a glass fiber filter paper.
  • the organic electrolyte containing the additive is composed of an additive, a solid lithium salt electrolyte and an organic solvent, the mass fraction of the additive in the electrolyte is 0.5% to 2%, and the concentration of the solid lithium salt electrolyte in the organic solvent is 0.2 to 5 mol/ L, wherein the additive is anhydrous lithium nitrate;
  • the solid lithium salt electrolyte is LiPF 6 , LiCF 3 SO 3 , LiN(CF 3 SO 2 ) 2 , LiClO 4 , LiP(C 6 H 4 O 2 ) 3 , LiPF 3 (C 2 F 5 ) 3 and a mixture of LiB(C 2 O 4 ) 2 in one or more ratios;
  • the organic solvent is 1,3-dioxol cyclopentane, ethylene glycol dimethyl ether, diethylene glycol One or a mixture of two or more kinds of ether solvents such as dimethyl ether, tetraethylene glycol dimethyl ether, 4-methyl-1,3-d
  • the preparation method of the positive electrode is: adding a conductive agent and a binder to the iodine element/carbon composite material, using water as a dispersing agent, adjusting the slurry, uniformly grinding and coating on a current collector (aluminum foil), under vacuum 80- After drying at 100 ° C, a positive electrode sheet was obtained.
  • the mass ratio of the conductive agent to the binder is 5-15% of the conductive agent, 5-10% of the binder, and the rest is the iodine element/carbon composite material.
  • the conductive agent is selected from at least one or a mixture of acetylene black, Super P, Vulcan XC-72, KS6, graphene, and carbon nanotubes.
  • the binder is composed of sodium carboxymethyl cellulose (CMC) and oil-filled styrene-butadiene rubber (SBR) binders mixed in different ratios, and the mass ratio is between 1:2 and 2:1.
  • CMC sodium carboxymethyl cellulose
  • SBR oil-filled styrene-butadiene rubber
  • the invention provides a long cycle life, high rate performance, low self-discharge effect and simple preparation of a cathode material
  • Organic electrolyte system lithium iodine secondary battery uses iodine element/carbon composite as the positive electrode.
  • the adsorption of iodine and its lithium salt by porous carbon effectively inhibits the dissolution of the active material, and at the same time improves the electrical conductivity of the electrode, showing better cycle performance and rate performance.
  • the ether electrolyte with the addition of anhydrous lithium nitrate was used to form a uniform protective film on the surface of the lithium by the reaction of anhydrous lithium nitrate with lithium metal, which reduced the self-discharge effect of the battery.
  • the iodine element/carbon composite material used is prepared by a room temperature "dissolution-adsorption" method, which does not require high-temperature heating to sublimate iodine, and does not cause loss of raw materials, and the iodine content of the prepared composite material is easy to control.
  • the preparation method provided by the invention has the advantages of simple and easy operation, safety, no pollution and strong practicability, and has wide application prospects.
  • Example 1 is a scanning electron micrograph of an iodine elemental/activated carbon cloth composite obtained in Example 1.
  • Example 2 is a thermogravimetric curve of the iodine elemental/activated carbon cloth composite obtained in Example 1.
  • Example 3 is an XPS spectrum of the iodine elemental/activated carbon cloth composite obtained in Example 1.
  • Example 4 is a graph showing a constant current charge and discharge curve at a rate of 0.5 C after standing, for 2 hours, 10 hours, and 24 hours after the battery assembled with the iodine elemental/activated carbon cloth composite obtained in Example 1.
  • Fig. 5 is a scanning electron micrograph of the negative electrode lithium sheet after the battery assembled by the iodine element/activated carbon cloth composite obtained in Example 1 was allowed to stand for 10 hours.
  • Fig. 6 is a graph showing the cycle charge and discharge capacity retention of a battery assembled of the iodine element/activated carbon cloth composite obtained in Example 1 at a rate of 0.5 C.
  • Fig. 7 is a graph showing the cycle charge and discharge capacity retention of batteries assembled by the iodine elemental/activated carbon cloth composite obtained in Example 1 at different magnifications.
  • Fig. 8 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine elemental/activated carbon cloth composite obtained in Example 2 at a rate of 0.5 C.
  • Fig. 9 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine element/activated carbon cloth composite obtained in Example 3 at a rate of 0.5 C.
  • Fig. 10 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine elemental/activated carbon cloth composite obtained in Example 4 at a rate of 0.5 C.
  • Figure 11 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine elemental/activated carbon cloth composite obtained in Example 5 at a rate of 0.5 C.
  • Fig. 12 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine elemental/activated carbon cloth composite obtained in Example 6 at a rate of 0.5 C.
  • Figure 13 is a scanning electron micrograph of the iodine element/CMK-3 composite obtained in Example 7.
  • Figure 14 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine element/CMK-3 composite obtained in Example 7 at a rate of 0.5 C.
  • Figure 15 is a graph showing the cycle charge and discharge capacity retention of a battery assembled of the iodine element/CMK-3 composite obtained in Example 7 at a rate of 0.5 C.
  • Fig. 16 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine element/CMK-3 composite material obtained in Example 8 at a rate of 0.5 C.
  • Figure 17 is a graph showing the constant current charge and discharge curves of a battery assembled of the iodine element/activated carbon composite obtained in Example 9 at a rate of 0.5 C.
  • Fig. 18 is a graph showing a constant current charge and discharge curve of a battery assembled of the iodine element/porous conductive carbon black composite obtained in Example 10 at a rate of 0.5 C.
  • Example 1 Preparation of iodine elemental/activated carbon cloth composite by room temperature "dissolution-adsorption" method, the steps are as follows:
  • the iodine elemental/activated carbon cloth composite material was obtained by filtration, washed three times with water, and dried at 80 °C.
  • the obtained sample was an iodine elemental/activated carbon cloth composite material, and its scanning electron microscope photograph is shown in Fig. 1.
  • Fig. 1 In order to determine the iodine content in the composite, it was subjected to a thermogravimetric test, and the resulting weight loss curve is shown in Fig. 2.
  • the measured mass fraction of iodine was 22%, corresponding to 5.6 mg/cm 2 .
  • the composite material was analyzed by X-ray photoelectron spectroscopy (model, AxisUltraDLD; instrument manufacturer, KratosAnalytical Ltd. UK) (XPS), and the obtained I3d spectrum is shown in Fig. 3.
  • Iodine was observed at 630.6 eV and 619.2 eV, respectively.
  • the characteristic peaks of elemental I3d 3/2 and I3d 5/2 demonstrate that a stable iodine element/activated carbon composite can be prepared by this simple "dissolution-adsorption" method.
  • the composite material prepared as described above was used as a positive electrode, the lithium metal plate was a negative electrode, and the organic electrolyte containing the additive was assembled in a glove box.
  • the electrolyte is a LiN(CF 3 SO 2 ) 2 solution having a concentration of 1.0 mol/L, and the solvent is a mixture of 1,3-dioxolane and ethylene glycol dimethyl ether in a volume ratio of 1:1, and the additive is Anhydrous lithium nitrate having a mass fraction of 1%.
  • the electrochemical performance of the electrode was tested as follows:
  • the voltage window was 2.0 to 3.6 V, and the obtained charge and discharge curve was obtained.
  • All specific capacities are calculated on the basis of the mass of iodine. It can be seen that the battery has almost no change in capacity after standing for a different time, and has reached 300 mAh/g, demonstrating a low self-discharge effect.
  • Fig. 5 is a scanning electron micrograph of the lithium negative electrode after standing for 10 hours, and the surface is relatively smooth.
  • Fig. 6 is a cycle life diagram of the electrode at a rate of 0.5 C.
  • the first discharge specific capacity is 299 mAh/g
  • the reversible specific capacity after 300 cycles is 200 mAh/g
  • the capacity retention rate is 67%
  • the Coulomb efficiency has been more than 90 percent.
  • the composite exhibits a high rate performance.
  • the electrode has reversible specific capacities of 301, 273, 232, and 169 mAh/g at 0.5 C, 1 C, 2 C, and 5 C, respectively, and exhibits high cycle stability at each current density. .
  • Example 2 The electrolyte in Example 1 was a LiN(CF 3 SO 2 ) 2 solution having a concentration of 1.0 mol/L, and the solvent was 1,3-dioxolane and ethylene glycol in a volume ratio of 1:1.
  • a mixture of methyl ether, the additive is 1% of anhydrous lithium nitrate changed to 1.0 mol/L of LiN(CF 3 SO 2 ) 2 solution, and the solvent is 1:1 dioxolan of 1:1 by volume.
  • the charge and discharge curves obtained at a magnification of 0.5 C are shown in Fig. 8.
  • Example 3 1.0 mol/L of LiN(CF 3 SO 2 ) 2 solution in Example 1 was prepared, and the solvent was a mixture of 1,3-dioxolane and ethylene glycol dimethyl ether in a volume ratio of 1:1.
  • the additive is a 1% by mass of anhydrous lithium nitrate changed to 1.0 mol/L of LiN(CF 3 SO 2 ) 2 solution, the solvent is tetraethylene glycol dimethyl ether, and the additive is anhydrous with a mass fraction of 1%.
  • Lithium nitrate, other simultaneous Example 1. The charge and discharge curves obtained at a magnification of 0.5 C are shown in Fig. 9.
  • Example 4 The amount of the iodine element added in Example 1 was determined to be 25 mg, and the same as in Example 1. The mass fraction of iodine in the obtained composite material was 11%, which corresponded to 2.5 mg/cm 2 . Using this composite material as a positive electrode, batteries were assembled in the same manner as in the examples, and a charge and discharge curve obtained at a magnification of 0.5 C is shown in FIG. It can be seen that the specific capacity obtained is much larger than the theoretical specific capacity of iodine. This is because the calculation of specific capacity is based on the mass of iodine. However, in the composite material, the content of iodine is relatively low, and the capacity contributed by the activated carbon cloth is relatively large.
  • Example 5 The amount of the iodine element added in Example 1 was set to 113 mg, and the same as in Example 1. The mass fraction of iodine in the obtained composite material was 36%, which corresponded to 11.6 mg/cm 2 . Using this composite material as a positive electrode, batteries were assembled in the same manner as in the examples, and a charge and discharge curve obtained at a magnification of 0.5 C is shown in FIG.
  • Example 6 The amount of the iodine element added in Example 1 was determined to be 169 mg, and the same as in Example 1. The mass fraction of iodine in the obtained composite material was 45%, which corresponded to 16.9 mg/cm 2 . Using this composite material as a positive electrode, batteries were assembled in the same manner as in the examples, and a charge and discharge curve obtained at a magnification of 0.5 C is shown in Fig. 12 .
  • Example 7 Preparation of iodine element/CMK-3 composite by room temperature "dissolution-adsorption" method, the steps are as follows:
  • the obtained sample was an iodine element/CMK-3 composite material, and a scanning electron microscope photograph thereof is shown in FIG.
  • the steps are as follows:
  • iodine element/CMK-3 composite material conductive carbon superP, binder sodium carboxymethyl cellulose (CMC) and oil-filled styrene-butadiene rubber (SBR) are mixed in water at a mass ratio of 80:10:5:5, and ground. After homogenization, the obtained slurry was applied to an aluminum foil, and dried at 80 ° C under vacuum to obtain an electrode sheet.
  • CMC carboxymethyl cellulose
  • SBR oil-filled styrene-butadiene rubber
  • the electrode sheet prepared above was used as a positive electrode, the lithium metal plate was a negative electrode, and an ether-based electrolyte containing an additive was used to assemble a battery in a glove box.
  • the electrolyte is 1.0 mol/L of LiN(CF 3 SO 2 ) 2 solution, and the solvent is a mixture of 1,3-dioxolane and ethylene glycol dimethyl ether in a volume ratio of 1:1, and the additive is a mass fraction. It is 1% anhydrous lithium nitrate.
  • the electrochemical performance of the electrode was tested as follows:
  • the assembled battery was tested for constant current charge and discharge at a rate of 0.5 C.
  • the voltage window was 2.0 to 3.6 V.
  • the characteristic charge and discharge curves are shown in Figure 14.
  • the corresponding cycle life diagram is shown in Figure 15.
  • the capacity after 100 cycles is cycled. There is still 128mAh/g.
  • Example 8 The amount of the iodine element added in Example 7 was determined to be 150 mg, and the same as in Example 7. The mass fraction of iodine in the obtained composite material was 60%. Using this composite material as a positive electrode, batteries were assembled in the same manner as in the examples, and a charge and discharge curve obtained at a magnification of 0.5 C is shown in FIG.
  • Example 9 The CMK-3 in Example 7 was changed to activated carbon, and the same as in Example 7. At a magnification of 0.5C The obtained charge and discharge curve is shown in Fig. 17.
  • Example 10 The CMK-3 in Example 7 was changed to a porous conductive carbon black (Ketjenblack, EC600JD), and the same as in Example 7. The charge and discharge curves obtained at a magnification of 0.5 C are shown in Fig. 18.
  • the invention provides an organic electrolyte system lithium iodine secondary battery and a preparation method thereof, which overcome the problems of serious self-discharge in the lithium ion iodine secondary battery of the organic electrolyte system and complicated preparation of the cathode material.
  • the iodine elemental/carbon composite material of the invention is prepared by a room temperature "dissolution-adsorption" method, does not require high temperature heating to sublimate iodine, does not cause loss of raw materials, and the iodine content of the prepared composite material is easy to control.
  • the adsorption of iodine and its lithium salt by porous carbon effectively inhibits the dissolution of the active material, improves the electrical conductivity of the electrode, and exhibits better cycle performance and rate performance.
  • the ether electrolyte with the addition of anhydrous lithium nitrate was used to form a uniform protective film on the surface of the lithium by the reaction of anhydrous lithium nitrate with lithium metal, which reduced the self-discharge effect of the battery.
  • the lithium iodine secondary battery of the organic electrolyte system of the invention has the characteristics of long cycle life, high rate performance, low self-discharge effect and strong practicability, and has low preparation cost, simple process, safety and pollution-free, and has wide application prospects.

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Abstract

La présente invention concerne une batterie secondaire au lithium-iode à système de solution électrolytique organique et un procédé de fabrication. La batterie comprend une électrode positive, une électrode négative, un séparateur et une solution électrolytique. Une matière active composite iode/carbone élémentaire est utilisée pour l'électrode positive. L'électrode négative est du métal lithium ou un alliage contenant du lithium. La solution électrolytique est une solution électrolytique d'ester contenant un additif nitrate de lithium anhydre. Il est utilisé un procédé de « dissolution-adsorption », dans lequel de l'iode élémentaire et une matière carbonée sont ajoutés dans une solution aqueuse et synthétisés par agitation. Avec la matière composite iode/carbone élémentaire comme électrode positive, la structure poreuse de la matière carbonée peut adsorber l'iode et autres sels de lithium, supprimant leur dissolution, et augmentant la stabilité de cycle. Dans le même temps, la grande conductivité électrique de la matière carbonée permet d'augmenter la performance des électrodes. L'additif nitrate de lithium anhydre dans la solution électrolytique peut réagir avec l'électrode négative pour former une couche de protection lisse, supprimant ainsi un effet d'auto-décharge de la batterie.
PCT/CN2015/086440 2015-05-06 2015-08-10 Batterie secondaire au lithium-iode à système de solution électrolytique organique et son procédé de fabrication WO2016176922A1 (fr)

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WO2019118409A1 (fr) * 2017-12-13 2019-06-20 Yale University Batteries rechargeables, électrodes métalliques de lithium, séparateurs pour batterie, et leurs procédés de fabrication et d'utilisation
CN113725414A (zh) * 2021-08-30 2021-11-30 郑州大学 一种水系锌碘二次电池正极材料及其正极和水系锌碘二次电池
CN114388868A (zh) * 2021-12-23 2022-04-22 南京大学 一种全固态锂-碘二次电池及其制备方法

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CN106848244A (zh) * 2017-02-28 2017-06-13 天津理工大学 一种有机电解液体系镁碘二次电池及其制备方法
KR101990618B1 (ko) * 2017-04-14 2019-06-18 주식회사 엘지화학 리튬 금속용 전기 도금용액 및 이를 이용한 리튬 금속전극의 제조방법
CN107666015B (zh) * 2017-09-04 2019-08-27 天津理工大学 一种水相电解质体系锌碘二次电池及其制备方法
CN110660990A (zh) * 2019-09-30 2020-01-07 河南工学院 碘基包合物二次电池正极及其制备方法及钠碘二次电池
CN114628710A (zh) * 2020-12-11 2022-06-14 中国科学院大连化学物理研究所 一种氟化碳电池用电解液及应用
CN112592538B (zh) * 2021-02-24 2021-05-14 苏州度辰新材料有限公司 一种塑料助剂预混物
CN113582231A (zh) * 2021-06-08 2021-11-02 湖南师范大学 一种MoO2/碳复合间层的制备方法
CN114335758B (zh) * 2021-12-31 2023-03-17 郑州大学 基于石榴石固态电解质高温熔融锂碘电池
CN114813795A (zh) * 2022-05-06 2022-07-29 南开大学 一种应用于电池材料研究的透射电镜双倾原位样品杆

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CN113725414A (zh) * 2021-08-30 2021-11-30 郑州大学 一种水系锌碘二次电池正极材料及其正极和水系锌碘二次电池
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CN114388868B (zh) * 2021-12-23 2023-10-13 南京大学 一种全固态锂-碘二次电池及其制备方法

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